Method of refining heavy mineral oils by means of sulphur dioxide in a continuous operation



April 11, 192s. 1,666,560

L. EDELEANU- ET AL IETHOD lOI R'EFINING HEAVYv MINERAL OILS BY MEANS OF SULPHUR DIOXIDE IN A CONTINUOUS OPERATION Filed Jun 25,l 1927 2 Sheets-Shoe?. 1

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April 17,1928. A 1,666,560

L. EDELEANU .ET AL METHOD OF-REFINING HEAVY MINERAL OILS.' BY MEANS OF `VSULPHUR DIOXI-DE IN A CONTINUOUS QPERATION Filed June 25. 192'? 2 Sheets-Sheet? 15 with SO deposes on the top.

. 3o 'to settle, after the as substantially um 50 ters, with constant PatenfedApr. 17, i928.

LAZABEDELEANU, m1

. mi. ennss, AND PAUL JonEcx, or BERLIN, annum. A

METHOD 0F G HEAVY IINEBAL OILS BY MEANS OF SULPHUR DIOXIDE IN -Y A CONTINUOUS OPERATION.

. .ihe invention relates to 'a process for rehiling heavy mineral oils by means of sulp ur '.lhisis a continuation in part of an application led September 13, 1924, Serial No.

` lt is already-known to refine light mineral oils by means of liquefied sulphur dioxide (SO2). In this process the sulphur dioxide i0 is. introduced from top to bottom and the oil to be relined rom bottom to top, *this counter-current resulting in the fact that the impurities saturated with SO2 (the extract) settle below,.whilst the puritied oil, mixed If heavy mineral oils are to .be refined, this process does not give a satisfying result. This resides in the fact that a mutual pene.- tration of the two liquids does not take place 20 in the desired extent due to the nature of the hea mineral oils; on the contrary, the liquefied SO, takes a few single -ways only through the oil so thatonly a portion of the latter comes in contact therewith, whilst the 25 other oil particles unacted upon.

. Consequently only individual quantities or charges' could be treated with SO2 by intimately the oil with the sulphur dioxide and causing the emulsion so formedA churn or agitator had been thrown out of backs the treatment Lof-individual charges suffers from in comparison with acontmuous operation are widely known and concern economy of the operation. the vpossibility has been perceived o f p mineral oils by a purely mec haincal-physica-l method by treating them with sulphur 40 also heavy mineral oils in-a vcontinuous operation like the light ones.

r Now the possibility has been found o renin also 'heavy mineral oils by the aid .of

` lique ed SO2 inlcontinuous operation, if the 5 mixing of the two liquids would-.be eected in a s ecial vessel provided with tor an by continuously sutpplying the emulsion so formed in regula quantities to. a

where the. emulsion enreduction 4of its velocity, within the so-called emulsion-zone, that is about in the The entrance in thesettlin rece tacle preferably takes .place centra y, wi an outward radial direction of Since settling receptacle,

dioxide in a continuous operation.v

' fined oil leaves the irst'settling receptacle,

bodiments of apparatus for car' g out the operation. The drawimproved process are illustra dioxide, a has been tries e purifyan agita- Application led June 25, 1927,1Scr1a1 No. 201,474, and in Germany June 12, 1924.

iiow, this causing the emulsion to spread in the settling receptacle uniformly from the center and with the lowest possible iiowing velocity. In this manner` the occasion is oered to the emulsion to separate according to the specific Weight of its constituents into extract and refined oil, these" two constituents, firstly still mixed with SOgthen being drawn oli on the top and bottom, re-

spectively.

The specific nature of the process enables to accomplishthe reiining operation in several stages. This may be performed by efecting the mixin 'in a plurality of special vessels having agitators, and by continuously -supplying the emulsions so formed to separate settling receptacles where they enter, with constantl reduction o their {iowing velocity and enter the so-called emulsionzone in a;v radial outward direction. The counter current principle is maintained therewith by the fact that the crude oil enters the last mixer, oxide enters the first one, and that the rewhilst the extract leaves the last one.

the 'intermediate stages the extract of the' preceding stage is always mixed with the refined oilzof the next stage.-

In the accompanying dra ngs some emexample.. In these drawings:

Fig. l is a vertical section through an apparatus for carrying out'the process in one sta e,- i

ig. is a detail thereof in enlargedscale, 'likewise in vertical section,

Fig. 3 is a somewhat modified arrangement of the apparatus of Fig. 1, in yertical section, v Fig. 4 is an apparatus according to Fig. 1 for carrying vout the process in several Fig. 5 is an apparatus according to Fig. 3, likewise for carrying out the process in several stages.

As to be seen from Fig. 1, the unit consists of a mixer 7 fitted with an agitator 6. The sulphur dioxide enters at 8 and the heavy mineral ture of oil and sulphur dioxidel enters the settlintgmreceptacle'll in tion ugh vthe pipe oil at 9. The intimate mixwhilst the pure sulphur diby way of continuous fopera.- 10 and eventually Y off at 13 and the extract at 1 regulated by a throttling means. The pipel preferably extends about to the midst of receptacle 11 and discharges the mixture i in radial directionl with the lowest possible speed' by means of a distributor 12. Thereby a continuous separation of extract and refmed oil takes place in a manner that uninterruptedly therrelined oil can be drawn Fig. 2 shows in enlarged scale an embodiment of the distributor 12.- As to be seen, the pipe 1() terminates in an annular slot 15 the cross section of vwhich gradually enlarges so that the mixture can flow out horizontally in all directions with a relatively low speed.

In the embodiment shown in Fig. 3 the 'mixer 7 is connected through a pipe 10 to an inclined settling receptacle 27 in such a manner that the emulsion enters-the socalled emulsion-zone with the lowest possible speed. This is obtained by a distributorv 12 which is of a construction as described on the hand of Fig. 2. The inclined position of the settling receptacle offers the advantage that the separation of rened oil and extract takes place more quickly than in a vertical receptacle. The refined product then leaves the settling receptacle at 13 again and the extract at 14. By providing pipe holes 28 in the settling receptacles 11 or 27 the operation can be controlled at any time j and regulated by adjusting the throttling members of pipe 10, so that the effect aimed at is really obtained. Y

Fig. 4 shows by way of example three units 16, 17, 18, each of whichA corresponds to the apparatus of Fig. 1. The units are connected in series and so arranged that the emulsion and the extract flow automatically,

due to gravity, from the one into the other receptacle, whilst the refined oil is pumped over. The sulphur dioxide arrives through 19 in the mixer of the first unit 16 and the oil to be refined arrives through 20 in the mixer ofthe last unit 18. The fresh sulphur dioxide is mixed with the refined oil of the second unit 17, this oil being pumped over through pipe l2l by means of a pump 22 into 'the mixer ofthe rst unit 16 whilst the extract of the rst unit Hows through pipe 33 into the mixer of the second unit where it is brought together' with the partly refined oil of the last .mixer that is pumped over Athrough pipe 23 by a pump 24. The partly refined oil'of the second.v unit enters; through pipe 34 the' mixer of' the third unit where it comes in contact with theoil to beirefined. Consequentlyv reined oil flows out continuously from the settling rece tacle of the first 16 at 25, and extract ows outcontinuously from the settling receptacle of the last unit 18 at 26.

Fig. 5' shows an apparatus consisting of three units 30, 31, 32 as shown in Fig. 3. The-How of the liquids is here the same as in the apparatus shown in Fig. 4, except that the extract too must be pumped over by pumps 29. 'Ihe pipes are denoted by the same reference numbers as in the embodiment of Fig. 4, and the direction of How of the liquids is indicated by arrows.`

What we claim as our invention and desire to secure by Letters-Patent, is

1. In a process for refining heavy mineral oils by means of sulphur dioxide in continuous operation: preparing an intimate mix.- ture of the oil and the sulphur dioxide in a vessel by means of a churning device, continuously supplying the mixture to a settling receptacle with a successively decreas ing speed and at a zone located about in the midst of the mixture already contained in said receptacle.

2. In a process orrelining heavy mineral oils by means of sulphur dioxide in continuous operation: preparing an intimate mixture of/the oil and the sulphur dioxide in a vessel by means of a churning device, continuously supplying the mixture to a settling receptacle with. a successively decreasing speed at a zone located about in the midst lof the mixture already contained in said reoutward direction.

3. In a process for refining heavy mineral oils by means of sulphur dioxide in continuous operation: preparing simultaneously a plurality of mixtures of the oil and the sulphur dioxide in a plurality of vessels by means of a plurality of churning devices, continuously supplying these mixtures each to a settling receptacle with a successively decreasing speed at a zone located about in the midst of the mixture already-contained in saidreceptacles, causing the mixture to enter saidv receptacles centrally andwith a radial outward direction, the` crude oil being supplied to the last and the pure sulphur dioxide being supplied to the rst of said plurality of vessels, whilst the refined oil leaves the first and the extract the last of said plurality of settling receptacles, the vessels locatedbetween said first and last vessel being ing and wlth the refined oil of the next stage.

- LAZAR EDELEANU. KARL PFEIFFER. KARL GRESS. PAUL JODECK. 

